HRID465254
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In 50 ml of methylene chloride is dissolved 19 g of methyl 2-hydroxyiminoacetoacetate and under ice-cooling and stirring 19.6 g of sulfuryl chloride is added dropwise. The mixture is stirred at room temperature for 3 days, after which the methylene chloride is distilled off under reduced pressure. The residue is dissolved in 200 ml of ether and washed seven times with 100 ml portions of water. The ether layer is dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 20.2 g of methyl 4-chloro-2-hydroxyiminoacetoacetate as a light-yellow oil.
WORKUP
后处理
- temperatureunder ice-cooling
- additionis added dropwise
- distillationafter which the methylene chloride is distilled off under reduced pressure
- dissolutionThe residue is dissolved in 200 ml of ether
- washwashed seven times with 100 ml portions of water
- dry with materialThe ether layer is dried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure